CN114471845A - Silica grinding method - Google Patents
Silica grinding method Download PDFInfo
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- CN114471845A CN114471845A CN202210139466.4A CN202210139466A CN114471845A CN 114471845 A CN114471845 A CN 114471845A CN 202210139466 A CN202210139466 A CN 202210139466A CN 114471845 A CN114471845 A CN 114471845A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 351
- 238000000227 grinding Methods 0.000 title claims abstract description 177
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000000498 ball milling Methods 0.000 claims abstract description 85
- 239000000843 powder Substances 0.000 claims abstract description 53
- 238000011049 filling Methods 0.000 claims abstract description 33
- 239000003960 organic solvent Substances 0.000 claims abstract description 31
- 239000002002 slurry Substances 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000002689 soil Substances 0.000 claims abstract description 15
- 238000003801 milling Methods 0.000 claims abstract description 13
- 238000007670 refining Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 19
- 238000007873 sieving Methods 0.000 claims description 15
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 23
- 230000000694 effects Effects 0.000 description 15
- 239000000523 sample Substances 0.000 description 14
- 239000011229 interlayer Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002270 dispersing agent Substances 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000012488 sample solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 4
- 239000006059 cover glass Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920005646 polycarboxylate Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/22—Lining for containers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/24—Driving mechanisms
Landscapes
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Crushing And Grinding (AREA)
- Silicon Compounds (AREA)
Abstract
The application discloses a silica grinding method, relates to the technical field of silica ore refining treatment, and comprises the following steps: s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes; s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7-0.9; s3, grinding: the silica slurry is refined by multiple ball milling, and in the Nth ball milling, the ball diameter of the grinding ball is DNThe flow rate of the silica slurry is QNThe filling amount of the grinding balls is FNIn the (N + 1) th ball milling, the ball diameter of the milling balls is D（N+1）The flow rate of the silica slurry is Q（N+1）The filling amount of the grinding balls is F（N+1）The silica slurry is ground for a plurality of times in a segmented mode by serially connecting a plurality of grinding machines, fine grinding of the silica slurry is achieved by adjusting the ball diameter of the grinding balls of each ball-grinding pass, the diameter-thickness ratio of silica is obviously improved, and the particle size of amorphous silica particles in the silica slurry is effectively reduced.
Description
Technical Field
The application relates to the field of silica processing, in particular to a silica grinding method.
Background
Silica is a non-metallic mineral product, which is a collection of minerals, mainly quartz, containing a certain amount of clay. The micro powder product prepared by processing the silica is very suitable to be used as a filler in rubber and plastic production. The superfine quartz powder is used as the rubber and plastic filler, so that the product cost can be obviously reduced, the processability of rubber can be improved, and the rubber and plastic filler has a good market prospect.
Generally, the finer the particle size of the quartz powder, the higher the filling rate in the polymer and the better the use effect. However, the pulverization and refinement of silica minerals cannot pursue fineness at once, and it is worth to retain natural lamellar structures of silica minerals as much as possible. The best refining effect of the silica mineral is to peel off the lamellar structure along the bedding surface, so that the radius-thickness ratio in the silica powder is larger. However, in the current silica refining process, an effective means is lacked to achieve the effect.
Disclosure of Invention
In order to reduce the refined granularity radius of the silica and improve the lamella diameter-thickness ratio in the silica, the application provides a silica grinding method.
The application provides a method for grinding silica, which adopts the following technical scheme:
a silica grinding method comprises the following steps: s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes; s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7-0.9; s3, grinding: performing ball milling and refining on the silica slurry for multiple times;
in the Nth ball milling, the ball diameter of the grinding balls is DN, the flow rate of the silica slurry is QN, and the filling amount of the grinding balls is FNIn the (N + 1) th ball milling, the ball diameter of the milling balls is D(N+1)The flow rate of the silica slurry is Q(N+1)The filling amount of the grinding balls is F(N+1)：
D(N+1)＝DN*QN*FN*P/(Q(N+1)*F(N+1))
Wherein P is the sieving proportion of the silica slurry after the first ball milling, FN≥F(N+1)，QN≥Q(N+1)。
By adopting the technical scheme, two mills are connected in series to grind the silica mineral aggregate, and raw materials with the same fineness are ground according to the grinding ball proportion and sequence with different fineness to obtain different effects. On one hand, the silica powder is prepared into silica slurry, the interaction force among the silica powder is reduced by adopting a wet grinding mode, and the lamellar structure in the silica powder is prevented from being broken due to excessive impact among particles in the grinding process. On the other hand, amorphous SiO contained in a silica slurry is ground by using divided grinding in a tandem grinding system2And (4) grinding the particles.
In the scheme, more important is the setting of the ball diameter of the grinding ball in the two ball-milling grinding processes. Firstly, the particles in the silica slurry are more effectively scattered and separated through the first ball milling with larger ball diameter. Meanwhile, the large spherical diameter also avoids the excessive breakage of the lamellar structure. In the second ball milling, the amorphous SiO is favorably milled by a smaller ball diameter of the milling ball2The particles are further refined and ground into spherical SiO2And (3) granules.
Optionally, D in S3N2.5-3.0mm, D(N+1)The minimum sphere diameter of (2.5 mm).
By adopting the technical scheme, practical tests show that D is obtainedNIn the interval of 2.5-3.0mm, if D(N+1)Less than 2.5mm, the preservation rate of the lamellar structure is reduced more.
Optionally, D in S3N2.0-2.5mm, D(N+1)Has a minimum sphere diameter of 2 mm.
By adopting the technical scheme, practical tests show that D is obtainedNIn the interval of 2.0-2.5mm, if D(N+1)Less than 2.0mm, the retention rate of the lamellar structure is reduced more.
Optionally, the rotation speed of the ball mill in S3 is 25-40 r/min.
By adopting the technical scheme, the rotating speed of 25-40r/min is kept, so that the silica grinding efficiency is ensured on one hand, and the grinding effect is also ensured on the other hand.
Optionally, in S3, the silica is ground twice, and the silica slurry in the first ball mill is heated to 70-80 ℃.
By adopting the technical scheme, the activity of the particles in the silica slurry is enhanced by heating the silica slurry, the distance between the particles is increased, and the grinding effect of the silica is obviously improved.
Optionally, cooling the silica slurry between the first ball milling and the second ball milling to 5-15 ℃.
By adopting the technical scheme, the expansion with heat and contraction with cold principle is utilized, the gap between the lamellar structure and the amorphous structure in the silica is increased, the dispersion of particles in the silica slurry is further improved, and the grinding effect of the secondary ball milling is obviously improved.
Optionally, in S3, Q1 is 0.6-0.7t/h, and Q2 is the same as Q1.
By adopting the technical scheme, the grinding efficiency of the silica slurry is improved.
Optionally, in S3, F1 is (0.7-0.9) × Q1.
Through adopting above-mentioned technical scheme, set for the packing volume of ball in order to improve the grinding effect.
Optionally, in S3, real-time currents of the mill during the first ball milling and the second ball milling are monitored, a stable current at an initial stage of starting the mill is taken as a calibration current, and if the real-time current is lower than the calibration current, the mill balls are added until the real-time current reaches the calibration current.
Through adopting above-mentioned technical scheme, the loss can appear at the grinding ball in grinding process, and the loss of grinding ball can make the load of mill descend, and the performance shows to descend for real-time current. In order to ensure the grinding effect, the loss of the grinding balls is monitored in a current monitoring mode, and the grinding balls are added in real time to ensure the grinding effect.
Alternatively, the grinding balls used in S3 are zirconium balls.
By adopting the technical scheme, the zirconium ball has the advantages of high hardness, high specific gravity, low abrasion and the like, and is favorable for improving the grinding effect of silica.
In summary, the present application includes at least one of the following benefits:
1. a plurality of mills are connected in series to grind the silica slurry for multiple times in a segmented manner, and the fine grinding of the silica slurry is realized by adjusting the ball diameter of a grinding ball in each ball-grinding pass, so that the diameter-thickness ratio in the silica is obviously improved;
2. the temperature of the ground silica is controlled, and the dispersion of particles in the silica is remarkably improved by using a temperature control system, so that the grinding effect of the silica is ensured;
3. the ball milling effect of the silica slurry is ensured by monitoring the current of the mill in real time to prevent and control the loss of the milling balls in the ball milling process.
Drawings
1. FIG. 1 is a schematic diagram of a polishing system according to the present application.
Reference numerals:
1. a feed pipe; 2. grinding the tank body; 3. a discharge pipe; 4. grinding the motor; 5. and (5) a transfer tank.
Detailed Description
The silica raw material adopted in the application is from silica ore of Zhangzhou, Fujian, of the company, and the organic solvent used in the application is a mixture of about 0.5% by weight of ACUMER 9400 (polycarboxylate dispersant with solid content of 40%), 6% of KH550, 15% of 75% ethanol and 78.5% of water. The grinder in this application is as shown in figure 1, and inlet pipe 1 is connected in the lower part of the grinding tank body 2, and discharging pipe 3 is connected in the upper portion of the grinding tank body 2, and grinding motor 4 is installed at the top of the grinding tank body 2. The prepared silica slurry enters the grinding tank body 2 from the lower part of the grinding tank body 2, and the grinding motor 4 drives the grinding blade to drive the grinding ball to grind the silica slurry in the grinding tank body 2. The ground silica slurry flows out of the discharge pipe 3 to the transfer tank 5 along with the continuous feeding of the silica slurry into the grinding tank body 2.
Example 1
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after primary ball milling, cooling to 10 ℃ through heat exchange, and introducing for secondary ball milling.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The ball diameter of the grinding balls was 3 × 0.625 × 0.5 × 95%/(0.625 × 0.5) ═ 2.85 mm.
The rotating speeds of the first ball mill and the second ball mill are both 30 r/min.
During the grinding process, the real-time current of the grinder is monitored, the current of the grinder during the first grinding is taken as the standard current, and when the current is lower than the standard current, grinding balls are added into the grinder until the real-time current reaches and is maintained at the standard current.
Example 2
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after primary ball milling, cooling to 10 ℃ through heat exchange, and introducing for secondary ball milling.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The grinding balls have a ball diameter of 3 × 0.625 × 0.5 × 95%(0.625 × 0.5) ═ 2.85 mm. The amount of sieving was 95%.
The silica slurry was subjected to a second ball milling and then to a third ball milling in which the silica slurry flow rate was 0.625t/h, the loading of the milling balls was 0.5t, and the ball diameter of the milling balls was 2.85 × 0.625 × 0.5 × 95%/(0.625 × 0.5) ═ 2.7 mm.
The rotating speeds of the ball mills of the first time, the second time and the third time are all 30 r/min.
Example 3
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 70 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after primary ball milling, cooling to 10 ℃ through heat exchange, and introducing for secondary ball milling.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The ball diameter of the grinding balls was 3 × 0.625 × 0.5 × 95%/(0.625 × 0.5) ═ 2.85 mm. The rotating speeds of the first and second ball mills are both 30 r/min.
Example 4
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 60 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after primary ball milling, cooling to 10 ℃ through heat exchange, and introducing for secondary ball milling.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The ball diameter of the grinding balls was 3 × 0.625 × 0.5 × 95%/(0.625 × 0.5) ═ 2.85 mm.
The rotating speeds of the first ball mill and the second ball mill are both 30 r/min.
Example 5
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after primary ball milling, cooling to 15 ℃ through heat exchange, and introducing for secondary ball milling.
In the second ball milling, the flow rate of the silica slurry was 0.625t/h, the loading of the milling balls was 0.5t, and the ball diameter of the D milling balls was 3 × 0.625 × 0.5 × 95%/(0.625 × 0.5) — 2.85 mm. The rotating speeds of the first and second ball mills are both 30 r/min.
Example 6
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after the first ball milling, cooling to 20 ℃ through heat exchange, and introducing into a second ball milling.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The ball diameter of the grinding balls was 3 × 0.625 × 0.5 × 95%/(0.625 × 0.5) ═ 2.85 mm. The rotating speeds of the first and second ball mills are both 30 r/min.
Example 7
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is subjected to ball milling and refining twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃;
in the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, D2The ball diameter of the grinding balls was 3 × 0.625 × 0.5 × 95%/(0.625 × 0.5) × 2.85 mm. The rotating speeds of the first and second ball mills are both 30 r/min.
Comparative example 1
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and the sieving amount of the silica slurry is 95%.
In the second ball milling, the flow rate of the silica slurry was 0.625t/h, the filling amount of the milling balls was 0.5t, and the ball diameter of the D milling balls was 3.2 mm. The rotating speeds of the first and second ball mills are both 30 r/min.
Comparative example 2
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after primary ball milling, cooling to 15 ℃ through heat exchange, and introducing for secondary ball milling.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The diameter of the grinding ball was set to 3.2 mm. The rotating speeds of the first and second ball mills are both 30 r/min.
Comparative example 3
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is subjected to ball milling and refining twice,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃;
and (3) introducing the silica slurry into a cooling tank with an interlayer after primary ball milling, cooling to 15 ℃ through heat exchange, and introducing for secondary ball milling.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D1The diameter of the grinding ball was set to 3.2 mm.
In the third ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The diameter of the grinding ball was set to 3.4 mm. The rotating speeds of the ball mills in the first time, the second time and the third time are all 30 r/min.
Performance detection test:
sample preparation: the silica slurries obtained in examples 1 to 7 and comparative examples 1 to 3 were sampled, respectively.
Sedimentation classification, calculating the size of particles by measuring the sedimentation velocity of the particles in a proper medium in a sample, carrying out sedimentation classification in a dilute suspension to ensure that solid particles in the suspension can be freely settled without mutual interference, calculating the sedimentation velocity according to a Stokes relation formula, and dividing the sample into five grades of 0-1 μm, 1-5 μm, 5-10 μm, 10-20 μm and more than 20 μm.
The particle size of each grade of particles in the sample was determined by a laser particle sizer.
And (3) measuring the thickness of the wafer layer in the sample wafer by adopting a half-lamination method:
1. adding 0.1g of sample into 10ml of distilled water to prepare a sample solution with the concentration of 1%, and uniformly stirring to fully disperse the particles;
2. removing a cover glass as a carrier, dripping a certain amount of dispersed sample solution on the cover glass by using a rubber head dropper, naturally flattening the sample solution on the glass slide, placing the glass slide on a test bench, standing until the sample solution is dried, and spreading each sample on the cover glass after the sample solution is dried;
3. the sample is sandwiched between two cover slips by dropping the universal glue on the tiled sample and then covering the top with a cover slip. After the sample was dried, the sample was broken from the middle, and the thickness of the sample sandwiched in the end face of the sample was observed under a scanning electron microscope.
The final data obtained by testing examples 1-7, comparative examples 1-3 are given in the following table:
according to the data of the two tables, the diameter-thickness ratio of the silica powder is obviously improved after multi-pass grinding, and the particle size is superior to that of other schemes.
Example 8
A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined for three times,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃; a heating jacket is arranged in the discharge pipe 3, and the silica slurry is heated by the heating jacket when flowing out of the discharge pipe 3, and the temperature of the silica slurry is heated and kept to 87-92 ℃. The silica slurry flows into the transfer tank 5 through a filter screen arranged at the top of the transfer tank 5. The outer side wall of the transfer tank 5 is provided with a cooling interlayer, and the silica slurry is cooled to 5 ℃ in the transfer tank 5 through heat exchange.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The ball diameter of the grinding balls was 3 × 0.625 × 0.5 × 95%/(0.625 × 0.5) ═ 2.85 mm.
The rotating speeds of the first ball mill and the second ball mill are both 30 r/min.
In the third ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D3The ball diameter of the grinding balls was 2.85 × 0.625 × 0.5 × 95%/(0.625 × 0.5) ═ 2.7 mm.
The rotating speed of the ball mill is 30 r/min.
During the milling process, the viscosity of the silica slurry flowing out of the second milling was monitored. The viscosity of the silica increased with the increase in silica fineness due to the two ball milling. Before the silica slurry is sent to the third grinding, a dispersant is added to reduce the viscosity of the silica slurry, so that the viscosity of the silica slurry is kept close to that of the silica slurry in the first grinding. The dispersant is one or the mixture of two of polycarboxylate dispersant and phosphate dispersant.
During the grinding process, the real-time current of the grinder is monitored, the current of the grinder during the first grinding is taken as the standard current, and when the current is lower than the standard current, grinding balls are added into the grinder until the real-time current reaches and is maintained at the standard current.
Comparative example 4:
a silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7;
s3, grinding: the silica slurry is ball milled and refined for three times,
in the first ball milling, the ball diameter of the grinding balls is 3mm, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, the sieving amount of the silica slurry is 95%, and the ball milling temperature is controlled at 75 ℃.
In the second ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D2The ball diameter of the grinding ball is 3 mm.
In the third ball milling, the flow rate of the silica slurry is 0.625t/h, the filling amount of the grinding balls is 0.5t, and D3The ball diameter of the grinding ball is 3 mm.
The rotating speed of the ball mill is 30 r/min.
The sample pieces in example 8 and comparative example 4 were taken for particle size detection analysis, and the particle size distribution in example 8 was as follows:
particle size distribution in comparative example 4:
as can be seen from the above table data, the silica slurry ground by the method in example 8 is more concentrated in the fineness distribution, so that the application characteristics of silica are more excellent. The reason is that the ball diameter of the grinding ball is gradually and properly reduced under the three-time grinding process, so that the particles in the silica slurry are more suitable for grinding environment. Meanwhile, the viscosity of the silica slurry is continuously increased along with the increase of the grinding times, the viscosity of the silica slurry is reduced by adding the dispersing agent, and the grinding effect is obviously improved.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. A silica grinding method is characterized by comprising the following steps:
s1, coarse crushing of raw ore: crushing and coarsely grinding a silica raw material to prepare silica powder smaller than 325 meshes;
s2, preparing slurry soil: mixing silica powder and an organic solvent to prepare slurry, wherein the weight ratio of the silica powder to the organic solvent is 1: 0.7-0.9;
s3, grinding: the silica slurry is subjected to ball milling and refining for a plurality of times,
in the Nth ball milling, the ball diameter of the grinding balls is DNThe flow rate of the silica slurry is QNThe filling amount of the grinding balls is FN,
In the (N + 1) th ball milling, the ball diameter of the milling balls is D（N+1）The flow rate of the silica slurry is Q（N+1）The filling amount of the grinding balls is F（N+1），
D（N+1） = （DN*QN*FN*P）/Q（N+1）*F（N+1）
Wherein P is the sieving proportion of the silica slurry after the first ball milling, FN≥F（N+1），QN≥Q（N+1）。
2. The silica grinding method according to claim 1, characterized in that: in S3DN2.5-3.0mm, DNHas a minimum sphere diameter of 2 mm.
3. The silica grinding method according to claim 2, characterized in that: in S3DN2.0-2.5mm, D（N+1）Has a minimum sphere diameter of 2 mm.
4. A silica grinding method according to claim 3, characterized in that: in S3, the rotation speed of the ball mill is 25-40 r/min.
5. The silica grinding method according to claim 1, characterized in that: in S3, the silica is ground twice, and the temperature of the silica slurry in the first ball milling is controlled to 70-80 ℃.
6. The silica grinding method according to claim 5, wherein: cooling the silica slurry between the first ball milling and the second ball milling to 5-15 ℃.
7. The silica grinding method according to claim 6, wherein: in S3, Q10.6-0.7t/h, Q2And Q1The same is true.
8. The silica grinding method according to claim 7, wherein: in S3, F1Is (0.7-0.9) Q1。
9. The silica grinding method according to claim 8, wherein: and in S3, monitoring the real-time current of the mill in the first ball milling and the second ball milling, taking the stable current at the initial starting stage of the mill as the calibration current, and if the real-time current is lower than the calibration current, adding the grinding balls until the real-time current reaches the calibration current.
10. The silica grinding method according to claim 9, wherein: the grinding balls used in S3 were zirconium balls.
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